CN115744962A - CuF 2 And method for preparing the same - Google Patents
CuF 2 And method for preparing the same Download PDFInfo
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- CN115744962A CN115744962A CN202211506386.4A CN202211506386A CN115744962A CN 115744962 A CN115744962 A CN 115744962A CN 202211506386 A CN202211506386 A CN 202211506386A CN 115744962 A CN115744962 A CN 115744962A
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- 229910016509 CuF 2 Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 103
- 239000007789 gas Substances 0.000 claims abstract description 51
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 50
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 24
- 239000011261 inert gas Substances 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 8
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006073 displacement reaction Methods 0.000 abstract description 3
- 238000007086 side reaction Methods 0.000 abstract description 3
- 229910052717 sulfur Inorganic materials 0.000 abstract description 3
- 239000011593 sulfur Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 8
- 239000010949 copper Substances 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000012265 solid product Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- 229910021594 Copper(II) fluoride Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- GWFAVIIMQDUCRA-UHFFFAOYSA-L copper(ii) fluoride Chemical compound [F-].[F-].[Cu+2] GWFAVIIMQDUCRA-UHFFFAOYSA-L 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- -1 transition metal salt Chemical class 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910018503 SF6 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 1
- 229960000909 sulfur hexafluoride Drugs 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a CuF 2 The preparation method comprises the steps of firstly, placing copper powder in a closed container, and introducing nitrogen or inert gas until air in the reaction container is completely discharged; feeding SF into the reaction vessel 6 Gas and make SF 6 Reacting the gas with the copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 630-690 ℃; SF 6 After the reaction of the gas and the copper powder is finished, cooling the reaction system, introducing nitrogen or inert gas into the reaction system at the same time until the temperature of the reaction system is reduced to room temperature to prepare the CuF 2 . The method enables copper powder to be mixed with SF 6 The gas directly generates displacement reaction at high temperature to generate CuF 2 The sulfur is gasified with the elemental sulfur to directly obtain CuF with higher purity 2 . Before and after the reaction, nitrogen or inert gas is adopted for protection, so that side reaction is avoided, the purity of the product is ensured, and a reaction system is safer.
Description
Technical Field
The invention belongs to the technical field of inorganic materials, and relates to CuF 2 And a method for preparing the same.
Background
With the demand of lithium batteries increasing sharply, cuF 2 Due to extremely high theoretical voltage, low price and low toxicity, the material can be used as an important lithium battery anode material. Preparation of CuF 2 The method mainly comprises a liquid phase method, a solvothermal method, a vapor deposition method and the like, for example, the liquid phase method is utilized by Liu Ximing and the like to prepare CuF 2 The method uses transition metal salt and alkali to react to generate corresponding hydroxide, and then HF is added to react with the hydroxide to generate CuF 2 Finally, excess reactant is removed by evaporation to yield CuF 2 (ii) a Thoralf Krahl et al solvothermally react copper alkoxides with HF at-70 ℃ to give CuF 2 (ii) a Brian Burrows et al obtained CuF deposited on the surface of an electrode by direct oxidation of a copper electrode with dry HF gas by vapor deposition under energized conditions 2 . At present, the preparation method of the copper fluoride in the laboratory mainly uses highly toxic HF highly active fluoride as a fluorine source, and not only strips are preparedThe parts are harsh, highly toxic HF is used, the preparation method is dangerous, the product needs to be subjected to post-treatment to improve the purity of the product, the operation is complicated, and the laboratory requirement is high.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides CuF 2 And a preparation method thereof, thereby solving the problem of CuF synthesis in the prior art 2 The preparation conditions are strict, the operation is complex and the danger is high.
The invention is realized by the following technical scheme:
CuF 2 The preparation method comprises the following steps:
s1: putting the copper powder in a closed container, and introducing nitrogen or inert gas until the air in the reaction container is completely discharged;
s2: feeding SF into the reaction vessel 6 Gas and make SF 6 Reacting the gas with the copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 630-690 ℃;
S3：SF 6 after the reaction of the gas and the copper powder is finished, cooling the reaction system, introducing nitrogen or inert gas into the reaction system at the same time until the temperature of the reaction system is reduced to room temperature to prepare the CuF 2 。
Preferably, the inert gas comprises one of helium or argon.
Preferably, in the step S1, the introduction rate of the nitrogen gas or the inert gas is 80 to 100mL/min.
Preferably, in the step S1, the introduction time of the nitrogen gas or the inert gas is 20 to 40min.
Preferably, the purity of the copper powder is greater than 99%.
Preferably, in step S2, SF 6 The gas is introduced at a rate of 40-50 mL/min.
Preferably, in the step S2, SF is introduced into the reaction vessel 6 After the flow rate of the gas flow is stable, the reaction system is subjected to temperature programming treatment to enable SF 6 Gas and copper powder inThe reaction is carried out at elevated temperature.
Preferably, the temperature increase rate in the step S2 and the temperature decrease rate in the step S3 are both 10 ℃/min.
Preferably, in the step S2, the reaction time of the high-temperature reaction is 50 to 80min.
CuF 2 Prepared by the method.
Compared with the prior art, the invention has the following beneficial technical effects:
CuF 2 The method of making copper powder and SF 6 Directly carrying out displacement reaction on gas at high temperature, specifically copper simple substance and SF 6 Reacting to generate CuF 2 The sulfur is gasified with the elemental sulfur at the reaction temperature of 630-690 ℃ at the same time to directly obtain CuF with higher purity 2 。SF 6 The gas is nontoxic and safe to operate, and in addition, nitrogen or inert gas is adopted to protect the reaction in the early stage and the later stage of the reaction, so that the side reaction is effectively avoided, the purity of the product is ensured, and the reaction system is safer.
Furthermore, the introduction speed of nitrogen or inert gas is 80-100 mL/min, so that the air in the reaction system is discharged more fully.
Further, the introduction time of nitrogen or inert gas is 20-40 min, so that the air in the reaction system is effectively discharged.
Furthermore, the purity of the copper powder is more than 99%, and the purity of the product is effectively improved.
Further, SF 6 The gas is introduced at a speed of 40-50 mL/min, so that SF can be ensured 6 The gas and the copper powder are fully contacted and reacted.
Further, SF is introduced into the reaction vessel 6 After the flow rate of the gas flow is stable, carrying out temperature programmed treatment on the reaction system to ensure that SF 6 The reaction of the gas with the copper powder is more complete.
Furthermore, the cooling rate in the step S3 is 10 ℃/min, so that the stability of the product structure is ensured.
Further, in step S2, the reaction time of the high-temperature reaction is 50-80 min, so that SF is obtained 6 The gas and the copper powder fully react.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 illustrates the preparation of CuF according to the present invention 2 A schematic flow diagram of (a);
FIG. 2 is a graph of CuF prepared in example 2 of the present invention 2 X-ray diffraction (XRD) pattern of (a);
FIG. 3 shows CuF prepared in example 2 of the present invention 2 Scanning Electron Microscope (SEM) photograph of (a);
FIG. 4 is a graph of CuF prepared in example 2 of the present invention 2 EDS spectrum of (3).
FIG. 5 is a graph of CuF prepared in example 2 of the present invention 2 TG-DSC chart of (1).
Detailed Description
To make the features and effects of the present invention comprehensible to those skilled in the art, general description and definitions are made below with reference to terms and expressions mentioned in the specification and claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The theory or mechanism described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features defined herein as numerical ranges or percentage ranges, such as values, amounts, levels and concentrations, are for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to cover and specifically disclose all possible subranges and individual numerical values (including integers and fractions) within the range.
In this document, unless otherwise specified, "comprising," including, "" having, "or similar terms, shall encompass the meaning of" consisting of 8230, 8230%, "consisting of" and "consisting essentially of 8230; \8230, consist of," e.g., "A comprising a" shall encompass the meaning of "A comprising a and the other" and "A comprising only a".
In this context, for the sake of brevity, not all possible combinations of features in the various embodiments or examples are described. Therefore, as long as there is no contradiction between combinations of these technical features, any combinations of the technical features in the respective embodiments or examples may be made, and all possible combinations should be considered as the scope of the present specification.
As shown in FIG. 1, the present invention provides a CuF 2 The preparation method comprises the following steps:
s1: putting copper powder with the purity of more than 99% in a closed container, and introducing nitrogen or inert gas until air in the reaction container is completely discharged; wherein the inert gas comprises one of helium or argon.
S2: SF is introduced into the reaction vessel at a speed of 40-50 mL/min 6 After the flow rate of the gas flow is stable, the temperature of the reaction system is programmed to ensure that SF is heated 6 Reacting the gas with the copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 630-690 ℃, and the reaction time of the high-temperature reaction is 50-80 min.
S3：SF 6 After the reaction of the gas and the copper powder is finished, cooling the reaction system, introducing nitrogen or inert gas into the reaction system at the same time until the temperature of the reaction system is reduced to room temperature to prepare the CuF 2 . The temperature rise rate of the program in the step S2 and the temperature drop rate in the step S3 are both 10 ℃/min.
CuF in the invention 2 The preparation method of (1) is that copper powder is mixed with SF 6 Directly carrying out displacement reaction on gas at high temperature, specifically copper simple substance and SF 6 Reacting to generate CuF 2 The sulfur is gasified with the elemental sulfur at the reaction temperature of 630-690 ℃ to directly obtain CuF with higher purity 2 . In addition, the reaction is protected by nitrogen or inert gas in the early stage and the later stage of the reaction, so that the side reaction is effectively avoided, the purity of the product is ensured, and the reaction system is safer. Compared with the existing CuF 2 Compared with the preparation method, the method has the advantages of simple equipment, convenient operation, safe synthesis process, cheap and easily-obtained raw materials, and is suitable for preparing the copper fluoride in batches in a laboratory.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out under conventional conditions or conditions recommended by the manufacturers. The various starting materials used in the examples which follow, unless otherwise indicated, are conventional commercial products having specifications which are conventional in the art. In the description of the present invention and the following examples, "%" represents weight percent, "parts" represents parts by weight, and proportions represent weight ratios, unless otherwise specified.
Example 1
2g of copper powder (500 nm, 99.9% purity) was weighed into a ceramic crucible, nitrogen was continuously introduced into the tube furnace at a flow rate of 100mL/min until the air in the tube furnace was evacuated, and then SF was added 6 Slowly introducing gas into the tube furnace at a flow rate of 50mL/min, heating to 600 deg.C at a temperature rise rate of 10 deg.C/min after gas flow is stable, and maintaining for 60min to obtain high-purity copper powder and SF 6 The thermal decomposition reaction is sufficiently caused. After the reaction is finished, continuously introducing nitrogen as protective gas, cooling to room temperature, and collecting white CuF 2 Solid product 2.7 g, yield 79％。
Example 2
2g of copper powder (500 nm, purity 99.9%) was weighed into a ceramic crucible, nitrogen was continuously introduced into the tube furnace at a flow rate of 100mL/min until the air in the tube furnace was evacuated, and then SF was added 6 Slowly introducing gas into the reaction system at a flow rate of 50mL/min, heating to 660 ℃ at a heating rate of 10 ℃/min after the gas flow is stable, and preserving heat for 60min to ensure that the high-purity copper powder and the SF are mixed 6 The thermal decomposition reaction is sufficiently caused. After the reaction is finished, continuously introducing nitrogen as protective gas, cooling to room temperature, and collecting white CuF 2 The solid product was 3.0 g, yield 86%.
CuF obtained in this example 2 The XRD pattern of (A) is shown in FIG. 2, and it can be seen from FIG. 2 that phase composition analysis of the solid product by XRD shows that diffraction peaks at 2 theta angles of 27.7 DEG, 33.7 DEG, 50.1 DEG, 57.2 DEG and the like respectively correspond to WS 2 The diffraction peaks of (011), (110), (112) and (022) crystal planes (PDF # 09-0136) of (A) were found to be CuF 2 。
CuF obtained in this example 2 The SEM picture of (1) is shown in FIG. 3, and it can be seen from FIG. 3 that CuF prepared by the present invention 2 The appearance distribution is uniform, and the product has good uniformity.
CuF prepared in this example 2 The EDS spectrum of fig. 4 shows that Cu and F are contained only and the ratio is close to 1 2 。
To study CuF in the present invention 2 The generation mechanism of (D) is shown in FIG. 5, and the results are shown in FIG. 5 in the case of SF, which is obtained from the TG-DSC chart obtained by the comprehensive thermal analyzer (HCT-4) 6 Under the atmosphere, when the tungsten powder is heated from room temperature at the temperature rising rate of 5 ℃/min, the weight of the material is increased within the range of 572-783 ℃, the weight increasing rate is 38.3 percent, the maximum exothermic peak appears on a DSC curve at 653 ℃, and the fluorination reaction is Cu(s) + SF 6 (g)→CuF 2 The apparent activation energy of (S) + S (g) is 56KJ/mol, so that the activation energy of the reaction is effectively reduced and the reaction is promoted by regulating and controlling the temperature.
Example 3
2g of copper powder (500 nm, purity 99.9%) was weighed into a ceramic crucible, helium was continuously introduced into the tube furnace at a flow rate of 100mL/min until the air in the tube furnace was evacuated, and then SF was added 6 Slowly introducing gas into the tube furnace at a speed of 50mL/min, heating to 690 ℃ at a heating rate of 10 ℃/min after the gas flow is stable, and keeping the temperature for 60min to ensure that the high-purity copper powder and the SF are mixed 6 The thermal decomposition reaction is sufficiently caused. After the reaction is finished, continuously introducing helium gas as protective gas, cooling to room temperature, and collecting white CuF 2 The solid product was 2.8 g, yield 81%.
Example 4
This example provides a CuF 2 The preparation method comprises the following steps:
s1: putting copper powder with the purity of 99% in a closed container, and introducing nitrogen for 20min at a rate of 80mL/min to completely discharge air in the reaction container;
s2: SF was introduced into the reaction vessel at a rate of 40mL/min 6 After the flow rate of the gas flow is stable, carrying out temperature programming treatment on the reaction system, wherein the temperature programming rate is 10 ℃/min, so that SF is ensured 6 Reacting the gas with the copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 630 ℃, and the reaction time of the high-temperature reaction is 50min.
S3：SF 6 After the reaction of the gas and the copper powder is finished, cooling the reaction system, introducing nitrogen into the reaction system at the same time until the temperature of the reaction system is reduced to room temperature, wherein the cooling rate is 10 ℃/min, and obtaining the CuF 2 。
Example 5
The present example provides a CuF 2 The preparation method comprises the following steps:
s1: putting copper powder with the purity of 99% in a closed container, and introducing nitrogen for 25min at the rate of 85mL/min to completely discharge the air in the reaction container;
s2: SF was introduced into the reaction vessel at a rate of 44mL/min 6 After the flow rate of the gas flow is stable, carrying out temperature programming treatment on the reaction system, wherein the temperature programming rate is 10 ℃/min, so thatSF 6 Reacting the gas with the copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 650 ℃, and the reaction time of the high-temperature reaction is 60min.
S3：SF 6 After the reaction of the gas and the copper powder is finished, cooling the reaction system, and simultaneously introducing helium gas into the reaction system until the temperature of the reaction system is reduced to room temperature, wherein the cooling rate is 10 ℃/min, so as to prepare CuF 2 。
Example 6
This example provides a CuF 2 The preparation method comprises the following steps:
s1: putting copper powder with the purity of 99.9% in a closed container, and introducing nitrogen for 35min at the rate of 90mL/min to completely discharge the air in the reaction container;
s2: SF was introduced into the reaction vessel at a rate of 50mL/min 6 After the flow rate of the gas flow is stable, carrying out temperature programming treatment on the reaction system, wherein the temperature programming rate is 10 ℃/min, so that SF is ensured 6 Reacting the gas with the copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 670 ℃, and the reaction time of the high-temperature reaction is 70min.
S3：SF 6 After the reaction of the gas and the copper powder is finished, cooling the reaction system, and simultaneously introducing nitrogen into the reaction system until the temperature of the reaction system is reduced to room temperature, wherein the cooling rate is 10 ℃/min, thus preparing the CuF 2 。
Example 7
The present example provides a CuF 2 The preparation method comprises the following steps:
s1: putting copper powder with the purity of 99.9% in a closed container, and introducing argon for 40min at the rate of 100mL/min to completely discharge the air in the reaction container;
s2: SF was introduced into the reaction vessel at a rate of 50mL/min 6 After the flow rate of the gas flow is stable, carrying out temperature programming treatment on the reaction system, wherein the temperature programming rate is 10 ℃/min, so that SF (sulfur hexafluoride) is enabled to be 6 Reacting the gas with the copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 690 ℃, and the reaction time of the high-temperature reaction is 80min.
S3：SF 6 After the reaction of the gas and the copper powder is finished, cooling the reaction system, introducing argon into the reaction system at the same time until the temperature of the reaction system is reduced to room temperature, wherein the cooling rate is 10 ℃/min, and obtaining the CuF 2 。
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. CuF 2 The preparation method is characterized by comprising the following steps:
s1: putting the copper powder in a closed container, and introducing nitrogen or inert gas until the air in the reaction container is completely discharged;
s2: feeding SF into the reaction vessel 6 Gas and make SF 6 Reacting the gas with the copper powder at high temperature; wherein the reaction temperature of the high-temperature reaction is 630-690 ℃;
S3：SF 6 after the reaction of the gas and the copper powder is finished, cooling the reaction system, introducing nitrogen or inert gas into the reaction system at the same time until the temperature of the reaction system is reduced to room temperature to prepare the CuF 2 。
2. CuF according to claim 1 2 The method of (3), wherein the inert gas comprises one of helium or argon.
3. According to the claimSolution of CuF as defined in claim 1 2 The preparation method is characterized in that in the step S1, the introduction speed of nitrogen or inert gas is 80-100 mL/min.
4. CuF according to claim 1 2 The preparation method is characterized in that in the step S1, the introduction time of nitrogen or inert gas is 20-40 min.
5. CuF according to claim 1 2 The method for preparing (1), wherein the purity of the copper powder is greater than 99%.
6. CuF according to claim 1 2 Is characterized in that, in the step S2, SF 6 The gas is introduced at a speed of 40-50 mL/min.
7. CuF according to claim 1 2 Is characterized in that in the step S2, SF is introduced into the reaction vessel 6 After the flow rate of the gas flow is stable, the reaction system is subjected to temperature programming treatment to enable SF 6 The gas reacts with the copper powder at high temperatures.
8. CuF according to claim 7 2 The preparation method is characterized in that the temperature rise rate in the step S2 and the temperature drop rate in the step S3 are both 10 ℃/min.
9. CuF according to claim 1 2 The preparation method of (1) is characterized in that in the step (S2), the reaction time of the high-temperature reaction is 50-80 min.
10. CuF 2 Characterized in that it is obtained by the process according to any one of claims 1 to 9.
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| JPH09285719A (en) * | 1996-04-23 | 1997-11-04 | Mitsubishi Electric Corp | Gaseous sulfur hexafluoride recovering and regenerating device and mobile recovering and regenerating device |
| JP2011155037A (en) * | 2010-01-26 | 2011-08-11 | Kyushu Institute Of Technology | Etching test method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09285719A (en) * | 1996-04-23 | 1997-11-04 | Mitsubishi Electric Corp | Gaseous sulfur hexafluoride recovering and regenerating device and mobile recovering and regenerating device |
| JP2011155037A (en) * | 2010-01-26 | 2011-08-11 | Kyushu Institute Of Technology | Etching test method |
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| Title |
|---|
| 颜世宏 等: "稀土氧化物氟化反应过程的研究", 稀土, no. 04, pages 16 - 19 * |
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